A value determining method for a sulfonamide veterinary drug residual matrix reference material in pork

Abstract

A value determining method for a sulfonamide veterinary drug residual matrix reference material in pork is provided. The method includes a matrix reference material pretreatment step. The pretreatmentincludes (1) a step of extraction, namely adding an extracting solvent into a matrix reference material for target substance extraction, and allowing an obtained liquid supernatant to pass through ananhydrous sodium sulfate column to obtain an extract; and (2) a step of purification, namely a step of subjecting the extract obtained in the step (1) to water-bath rotary evaporation drying, addinga mobile phase to a constant volume to dissolve the extract; performing filtration through a liquid-liquid partition purification process and performing filtration to obtain the pretreated matrix reference material, wherein the anhydrous sodium sulfate column is infiltrated with acetonitrile in advance and the mobile phase is saturated with n-hexane in advance. The n-hexane-saturated mobile phaseis added to the extract of the sulfonamide veterinary drug residual matrix reference material to a certain volume, thus reducing distribution of sulfonamide drug in an extract liquid into an organic phase during liquid-liquid partition. The sulfonamide drug recovery rate is 95.7-104.8%, and the relative standard deviation is less than 5% (with n being 6).

Description

technical field [0001] The invention belongs to the technical field of analysis and detection, and relates to a value determination method for a matrix standard substance of sulfonamide veterinary drug residues in pork. Background technique [0002] Sulfonamide veterinary drugs are a general term for a class of antibacterial drugs with a sulfanilamide structure. They have the advantages of wide antibacterial spectrum, strong antibacterial ability, and low price. They are widely used in the prevention and treatment of infectious diseases in food-borne animals. However, long-term consumption of animal-derived foods containing sulfonamide veterinary drugs is likely to cause allergic reactions, affect the function of the urinary system, produce crystalluria, hematuria and other symptoms, destroy the ecological balance of the normal flora of the body, and cause adverse consequences such as bacterial resistance. Sulfa veterinary drugs are one of the veterinary drugs whose residues...

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Problems solved by technology

[0004] Liquid chromatography-tandem mass spectrometry (LC-MS / MS) is currently the main confirmation method for the detection of sulfonamides. However, due to the high fat content and protein content in pork, the pretreatment process is cumbersome, which significantly affects the reliability of the determination results. sex and accuracy

The standard recovery of LC-MS / MS reported in the literature is generally 70%-110%, and the standard deviation of the results is generally 15%-30%, which cannot meet the fixed value requirements of the matrix standard substance ("ultra high performance liquid chromatography-tandem Determination of sulfa drug residues in pork by mass spectrometry", Yang Mei et al., "Journal of Food Safety and Quality Inspection", Vol. 8, pp. 3633-3638, 2017)

[0005] CN 101949898 A discloses a method for detecting residues of various basic drugs in animal-derived foods. The method is extracted by vortexing and mixing acetonitrile, isopropanol and citric acid buffer solution, and hydrophilic polystyrene-diethylene Benzene solid-phase extraction column and cation-exchange solid-phase extraction column purification and liquid chromatography-mass spectrometry to detect a variety of basic drugs such as β-receptor agonists and sulfonamides in pork, pig liver, eggs, shrimp, and milk , benzodiazepines, nitroimidazoles, benzimidazoles, and triphenylmethane residues, but this method did not remove the water in the extraction solvent, which significantly affected the relative recovery and relative standard deviation of the drug. The relative recovery rate is only 63.1%-109.0%, and the relative standard deviation is 1.6%-23.0%, which cannot meet the value requirements of the matrix standard substance

[0006] CN 102175784 A discloses a method for the simultaneous determination of 54 drug residues in pork by solid-phase extraction-liquid chromatography-mass spectrometry / mass spectrometry. 18 Solid phase extraction cartridge cleanup, liquid chromatography-mass spectrometry / mass spectrometry (LC-MS / MS) determination, isotope internal standard dilution internal standard method and external standard method for quantification, the recovery range is 21.1%-121%, relative standard deviation less than 19.8%, it can be used as a screening method for the simultaneous determination of 54 drug residues in pork including sulfonamides, nitroimidazoles, quinolones, macrolides, lincosamides and praziquantel. Recovery and relative standard deviation still need to be further optimized

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